CN107641142A - The production technology of Chinese yam saponin in a kind of Hu Luba seeds - Google Patents
The production technology of Chinese yam saponin in a kind of Hu Luba seeds Download PDFInfo
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- CN107641142A CN107641142A CN201711026456.5A CN201711026456A CN107641142A CN 107641142 A CN107641142 A CN 107641142A CN 201711026456 A CN201711026456 A CN 201711026456A CN 107641142 A CN107641142 A CN 107641142A
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Abstract
The invention provides a kind of production technology of Chinese yam saponin in Hu Luba seeds, concretely comprise the following steps：(1) Hu Luba seeds are broken for particle using physical method；(2) plus non-polar solven to Hu Luba seed particles extract Hu Luba oil and recycling design；(3) additive polarity solvent to degreasing Hu Luba seed particles are extracted, and obtain supernatant and precipitation, and precipitation can be used as high protein feed；(4) concentrated supernatant；(5) solubilizer to concentrate makes contamination precipitation；(6) separation impurity obtains secondary supernatant；(7) recycling design and saponin is obtained from secondary supernatant, traditional acid hydrolysis process can be used to obtain Chinese yam saponin for gained saponin；The technique need not use UF membrane and resin column isolation technics; utilize dissolubility difference of the Hu Luba seed each components in different solvents; (or filtering) is extracted and centrifuged by multiple-stage solvent can isolate and purify saponin and other active ingredients, be adapted to the needs of scale industrial production.
Description
Technical field
The present invention relates to Chinese medicine separation-extraction technology, the production technology of Chinese yam saponin in especially a kind of Hu Luba seeds.
Background technology
Hu Luba is traditional Chinese medicine, and herb and seed are used as medicine, annual pulse family draft raise crop, also known as tonka-bean, hardship
Beans, cucurbit fragrant plant, foreign country is incoming, and title transliteration, alias is a lot of, what the Chinese Academy of Sciences edited and publish《Qinling Mountains flora》Name Hu Luba.
Hu Luba originates in West Africa, is passed to China through Mediterranean during Han dynasty, cultivates and be used as medicine first recorded in the Northern Song Dynasty《Jiayou Bencao》, there is temperature
The function such as kidney, dispelling cold, hypoglycemic, reducing blood lipid, analgesic.Hu Luba seeds use existing very long history as antidiabetic, to blood
Sugar has dual regulation, keeps the balance of body blood glucose, and this is that other hypoglycemic drugs are unexistent, and this effect is in recent years
Confirmed also to obtain the clinical of the country such as English, print, method.Modern study shows that the carpaine in Hu Luba seeds has significant anti-
Cancer activity, and rabbits blood pressure decline and vasodilation can be caused.Due to both at home and abroad to fenugrec and herb chemical composition,
The purposes of series of products, which is studied, must compare thoroughly, possess the basic condition of simple series exploitation and comprehensive utilization.Except medicinal
Outside, the composition that Hu Luba can be comprehensively utilized also includes Chinese yam saponin, vegetable oil and protein feed.
Steroid hormone medicine is synthesized based on the chemical framework of Chinese yam saponin, last century end the United Nations's health organization
Announced according to the clinical effectiveness of decades, prohibit the use of chemical synthesis to produce steroid hormone medicine, the Material synthesis of animal origin
Medicine causes side effect, also prohibits the use of, and therefore, plant is the unique raw material source of semi-synthetic steroid drugs.It is phase a few days ago, yellow
Ginger is the raw material for producing Chinese yam saponin, is the exclusive species in China, the Chinese yam saponin in China has monopolized international market.Due to yellow ginger
The raising of planting cost, stigmasterol (deriving from soybean) have the potentiality for substituting Chinese yam saponin, and Hu Luba seeds contain Chinese yam saponin, are to replace
For yellow ginger and the optimal plant resources of stigmasterol.
The unsaturated fatty acid content of Hu Luba oil is up to 82.48%, and its Linoleic acid accounts for more than 59%, can be used as medicine
The linoleic pharmaceutical raw material of product.Also it can be made into health products sale.In existing Hu Luba seeds extract saponin method mainly have with
Under it is several:
The A of patent application document CN 104784246 disclose in July, 2015 extracts saponin in a kind of seed from Hu Luba
Method, but this method needs to use macroporous absorbent resin separation saponin.This method is not suitable for saponin due to price reasons
The big production of industry.
The A of patent application document CN 104224894 disclose one kind in December, 2014 and extract saponin from Hu Luba seeds
Method, but this method needs multistage membrane filtration, be not suitable for the big production of industry of saponin.
The A of patent application document CN 101255183 are disclosed in September, 2008 and saponin are extracted in a kind of seed from Hu Luba
Method, but this method is equally also required to use macroporous absorbent resin, the big production of industry of saponin is not suitable for it.
Patent application document CN1456570 A disclose the side that saponin is extracted in a kind of seed from Hu Luba in November, 2003
Method, but this method is equally also required to use macroporous absorbent resin, the big production of industry of saponin is not suitable for it.
As fully visible, Hu Luba is a kind of industrial crops of good market prospect, and its seed contains saponin, height unsaturated oils
Fat and high quality protein.Existing process extractable refined Chinese yam saponin, vegetable oil and protein feed, but they are required for using
UF membrane or resin post separation.Under existence conditions, due to cost reason, UF membrane and resin post separation are difficult to apply at this
In the big production of industry of class product.Therefore, the comprehensive utilization of Hu Luba seeds is not yet by industrialization.Therefore, research and development it is a kind of without using
The extracting method of UF membrane and resin post separation, the comprehensive utilization of industrialization Hu Luba seeds is expected to, is had broad application prospects.
The content of the invention
The technical problems to be solved by the invention the Chinese yam saponin in a kind of Hu Luba seeds are provided production technology, same
Can be with the active ingredient of isolated a variety of Hu Luba seeds during one production.
In order to solve the above technical problems, the technical scheme is that：
The production technology of Chinese yam saponin, is concretely comprised the following steps in a kind of Hu Luba seeds：
(1) Hu Luba seeds are broken for particle using physical method；
(2) plus non-polar solven to Hu Luba seed particles extract Hu Luba oil and recycling design, the non-polar solven
It is 0.05-20 with Hu Luba seeds granular mass ratio：1；
(3) additive polarity solvent to degreasing Hu Luba seed particles are extracted, the polar solvent and degreasing Hu Luba seeds
The mass ratio of grain is 5-20:1, supernatant and precipitation are obtained, precipitation can be used as high protein feed；
(4) concentrated supernatant；
(5) solubilizer to concentrate makes contamination precipitation；
(6) separation impurity obtains secondary supernatant；
(7) recycling design and saponin is obtained from secondary supernatant, traditional acid hydrolysis process can be used to obtain for gained saponin
Chinese yam saponin.
Preferably, in above-mentioned Hu Luba seeds Chinese yam saponin production technology, the non-polar solven includes linear paraffin, props up
Alkane and its mixture, it is 4-12 to be related to molecule carbon atoms number scope.
Preferably, in above-mentioned Hu Luba seeds Chinese yam saponin production technology, the polar solvent include water, acetonitrile, methanol,
Ethanol and its mixture.
Preferably, in above-mentioned Hu Luba seeds Chinese yam saponin production technology, use polar solvent extraction degreasing Hu Luba seeds
The technique of particle includes ultrasound adverse current and extracted, and adverse current is extracted, agitation and filtration extraction.
Preferably, in above-mentioned Hu Luba seeds Chinese yam saponin production technology, the mass ratio of the concentrate and supernatant is
0.02-0.5:1。
Preferably, in above-mentioned Hu Luba seeds Chinese yam saponin production technology, it is described add concentrate solvent for water, second
Nitrile, methanol, ethanol, ethyl acetate, chloroform, n-hexane or its any mixture.
Preferably, in above-mentioned Hu Luba seeds Chinese yam saponin production technology, add the solvent of concentrate and the matter of concentrate
It is 1-9 to measure ratio:1.
Preferably, in above-mentioned Hu Luba seeds Chinese yam saponin production technology, comprise the following steps that:
(1) Hu Luba seed physics is broken into particle；
(2) plus non-polar solven to Hu Luba seed particles extract Hu Luba oil and recycling design, the non-polar solven
For linear paraffin, branched paraffin or the two mixture, it is 4-12 to be related to molecule carbon atoms number scope, the non-polar solven
It is 0.05-20 with Hu Luba seeds granular mass ratio：1；
(3) additive polarity solvent to degreasing Hu Luba seed particles are extracted, and obtain supernatant and precipitation, and precipitation can be used as height
Protein feed, the polar solvent are water, acetonitrile, methanol, ethanol or its mixture, the polar solvent and degreasing Hu Luba seeds
The mass ratio of particle is 5-20:1, the technique that degreasing Hu Luba seed particles are extracted using polar solvent includes ultrasound adverse current extraction,
Adverse current is extracted, agitation and filtration extraction；
(4) concentrated supernatant, gained concentrate is 0.02-0.5 with the mass ratio of supernatant：1；
(5) solubilizer to concentrate makes contamination precipitation, and the solvent for adding concentrate is water, acetonitrile, methanol, ethanol, acetic acid
Ethyl ester, chloroform, n-hexane or its mixture, the mass ratio of the solvent for adding concentrate and concentrate is 1-9：1；
(6) separation impurity obtains secondary supernatant；
(7) recycling design and saponin is obtained from secondary supernatant, traditional acid hydrolysis process can be used to obtain for gained saponin
Chinese yam saponin.
Preferably, in above-mentioned Hu Luba seeds Chinese yam saponin production technology, the non-polar solven is food-grade 6# solvents
When oily, the polar solvent of selection is water, and the solvent added in concentrate is absolute ethyl alcohol or 95% ethanol.
The beneficial effects of the invention are as follows：
The production technology of Chinese yam saponin in above-mentioned Hu Luba seeds, without UF membrane and resin column isolation technics is used, utilize
Dissolubility difference of the Hu Luba seed each components in different solvents, it is i.e. separable that (or filtering) is extracted and centrifuged by multiple-stage solvent
Saponin and other active ingredients are purified, are adapted to the needs of scale industrial production.
Brief description of the drawings
Fig. 1 is the production technological process of Chinese yam saponin in Hu Luba seeds of the present invention.
Embodiment
In order that those skilled in the art is better understood from technical scheme, it is below in conjunction with the accompanying drawings and specific real
Mode is applied to be described in further detail technical scheme of the present invention.
Embodiment 1
As shown in figure 1, in a kind of Hu Luba seeds Chinese yam saponin production technology, concretely comprise the following steps：
550 Ke Huluba seeds are broken into particle, with 1650ml food-grade 6# solvent naphthas, heating and refluxing extraction 8 hours, obtained
50 Ke Huluba oil and 500 grams of degreasing Hu Luba seed particles.By degreasing Hu Luba seeds particle with 12 times of water (6000 grams), in water
Ultrasound adverse current is extracted in the case of 45 DEG C of temperature, obtains 500 grams of extraction slags and 6000 grams of extract solutions.Extraction slag drying can do albumen feeding
Material.Extract solution is evaporated under reduced pressure to 1400 grams of concentrates.Add 4600 grams of absolute ethyl alcohols in concentrate, stir evenly, it is small to staticly settle 4
When, centrifuge, obtain 500 grams of sediments and 5500 grams of ethanol dissolved matters.Sediment can do protein feed in 80 DEG C of drying.Ethanol
Dissolved matter squeezes into distillation still recovery ethanol.Stop distillation when temperature reaches 100 DEG C when bottom, obtain 100 grams of saponin aqueous solution.By system
Take the traditional handicraft of Chinese yam saponin to operate, obtain 3.6 grams of Chinese yam saponins.
Embodiment 2
The production technology of Chinese yam saponin, is concretely comprised the following steps in a kind of Hu Luba seeds：
550 Ke Huluba seeds are broken into particle, with 1650ml food-grade 6# solvent naphthas, heating and refluxing extraction 8 hours, obtained
50 Ke Huluba oil and 500 grams of degreasing Hu Luba seed particles.By degreasing Hu Luba seeds particle with 13 times of water (6500 grams), in water
Ultrasound adverse current is extracted in the case of 45 DEG C of temperature, obtains 500 grams of extraction slags and 6500 grams of extract solutions.Extraction slag drying can do albumen feeding
Material.Extract solution is evaporated under reduced pressure to 1500 grams of concentrates.Add 5000 gram of 95% ethanol in concentrate, stir evenly, it is small to staticly settle 4
When, centrifuge, obtain 500 grams of sediments and 6000 grams of ethanol dissolved matters.Sediment can do protein feed in 80 DEG C of drying.Ethanol
Dissolved matter squeezes into distillation still recovery ethanol.Stop distillation when temperature reaches 100 degree when bottom, obtain 150 grams of saponin aqueous solution.By system
Take the traditional handicraft of Chinese yam saponin to operate, obtain 3.8 grams of Chinese yam saponins.
Embodiment 3
The production technology of Chinese yam saponin, is concretely comprised the following steps in a kind of Hu Luba seeds：
5 tons of Hu Luba seeds are broken into particle, use 15m3Food-grade 6# solvent naphthas, heating and refluxing extraction 8 hours, obtain 0.4
Ton Hu Luba oil and 4.6 tons of degreasing Hu Luba seed particles.Degreasing Hu Luba seed particles are transferred in ultrasonic countercurrent extraction machine and carried
Take, 45 DEG C of water temperature, 12 times of amount of water (55.2 tons), obtain 2.8 tons of extraction slags and 57 tons of extract solutions.Extraction slag drying can do albumen feeding
Material.Extract solution moves into evaporating kettle, is evaporated under reduced pressure to 13 tons of concentrates.Add 44 tons of absolute ethyl alcohols in concentrate, stir 30 minutes,
Staticly settle 4 hours, centrifuge, obtain 3 tons of sediments and 54 tons of ethanol dissolved matters.Sediment can do albumen feeding in 80 DEG C of drying
Material.Ethanol dissolved matter squeezes into distillation still recovery ethanol.Stop distillation when temperature reaches 100 degree when bottom, it is water-soluble to obtain 0.2 ton of saponin
Liquid.Traditional handicraft by Chinese yam saponin is produced operates, and obtains 0.035 ton of Chinese yam saponin.
As fully visible, compared with than in traditional handicraft：(1) Hu Luba seeds are crushed, sieves, separate film；(2) residue is taken off
Fat obtains vegetable oil；(3) 3 times of 1M hydrochloric acid solutions are added in degreasing thing, in 2kg/cm2Hydrolyzed 2 hours under pressure；(4) acid solution is filtered off,
Filter cake is washed with water to neutrality, drying, Chinese yam saponin is extracted with No. 120 industrial napthas.Chinese yam in Hu Luba seeds of the present invention
The production technology of saponin in the case where ensureing saponin yield, additionally can get Hu Luba oil, trigonella bean gun, protein feed etc. it is a variety of
Product.Because chromatographic isolation and UF membrane need not be used, in big production scale, production cost will be far below existing skill
Art, there is obvious superiority.
It is above-mentioned to be retouched in detail with reference to what embodiment was carried out to the production technology of Chinese yam saponin in a kind of Hu Luba seeds
State, be illustrative rather than limited, several embodiments can be included according to limited scope, therefore do not departing from this
Changing and modifications under invention general plotting, it should belong within protection scope of the present invention.
Claims (8)
- A kind of 1. production technology of Chinese yam saponin in Hu Luba seeds, it is characterised in that：Concretely comprise the following steps：(1) Hu Luba seeds are broken for particle using physical method；(2) plus non-polar solven to Hu Luba seed particles extract Hu Luba oil and recycling design, the non-polar solven and Hu Lu bar seed granular mass ratio is 0.05-20：1；(3) additive polarity solvent to degreasing Hu Luba seed particles are extracted, the polar solvent and degreasing Hu Luba seed particles Mass ratio is 5-20:1, supernatant and precipitation are obtained, precipitation can be used as high protein feed；(4) concentrated supernatant；(5) solubilizer to concentrate makes contamination precipitation；(6) separation impurity obtains secondary supernatant；(7) recycling design and saponin is obtained from secondary supernatant, traditional acid hydrolysis process can be used to obtain Chinese yam for gained saponin Saponin.
- 2. the production technology of Chinese yam saponin in Hu Luba seeds according to claim 1, it is characterised in that：It is described nonpolar molten Agent includes linear paraffin, branched paraffin and its mixture, and it is 4-12 to be related to molecule carbon atoms number scope.
- 3. the production technology of Chinese yam saponin in Hu Luba seeds according to claim 1, it is characterised in that：The polar solvent Comprising water, acetonitrile, methanol, ethanol and its mixture.
- 4. the production technology of Chinese yam saponin in Hu Luba seeds according to claim 1, it is characterised in that：Use polar solvent The technique for extracting degreasing Hu Luba seed particles includes ultrasound adverse current extraction, and adverse current is extracted, agitation and filtration extraction.
- 5. the production technology of Chinese yam saponin in Hu Luba seeds according to claim 1, it is characterised in that：The concentrate with The mass ratio of supernatant is 0.02-0.5:1.
- 6. the production technology of Chinese yam saponin in Hu Luba seeds according to claim 1, it is characterised in that：It is described to add concentration The solvent of liquid is water, acetonitrile, methanol, ethanol, ethyl acetate, chloroform, n-hexane or its any mixture.
- 7. the production technology of Chinese yam saponin in Hu Luba seeds according to claim 1, it is characterised in that：Add concentrate The mass ratio of solvent and concentrate is 1-9:1.
- 8. the production technology of Chinese yam saponin in Hu Luba seeds according to claim 1, it is characterised in that：It is described nonpolar molten When agent is food-grade 6# solvent naphthas, the polar solvent of selection is water, and the solvent added in concentrate is absolute ethyl alcohol or 95% second Alcohol.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113264977A (en) * | 2021-05-21 | 2021-08-17 | 周康 | Production process of diosgenin |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962686A (en) * | 2006-11-19 | 2007-05-16 | 王元华 | Method for cleanly producing saponin by integrated utilization of yam |
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2017
- 2017-10-27 CN CN201711026456.5A patent/CN107641142A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962686A (en) * | 2006-11-19 | 2007-05-16 | 王元华 | Method for cleanly producing saponin by integrated utilization of yam |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113264977A (en) * | 2021-05-21 | 2021-08-17 | 周康 | Production process of diosgenin |
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